Cocoa derivative and the process of separating constituents of the cacao-bean.



U r ran sraras ROBERT H- EZIIDDLE, QR RAH'WAY, NEW JEESEY, ASSIGNOR 0F THREE-FOUBTHS TO IAJEB, QENEW YORK, II. PROCESS OF SEPABATING COIlSTITUIE-UTS .OF-THE Patented-Sept. 16, 1913.

,,coco.a imnrvarivnaansrnn QACAO-BEAN.

1,97 3, 1% 'fineoificetion of Letters Patent. Ho Drawing.

Toall who m zit may concern:

,Be itknown that I, Ronnn'r N. RI DLE, a citizen of the United States, residing at Rahway, county of Union, State of New Jersey,'-ha ve invented a Cocoa Derivative and a Process ofSeparating Constituents of the 'Cacao Bean, of which the following is aspecification. I

The complete extraction of the cacao butter, or fat of the cacao-bean, and'of the alkaloids contained in the bean, is not efi'ected in'the, manufacture of cacao powder as at present practised, nor is it even attempted. The roasted and shelled cacao beans, broken-into the form of cacao nibs, are commonlyv ground between revolving heated stones so that; the cacao mass, be cause of the high per cent. of fat that. it contains, 'is melted and lows from the grinding stones at a temperature of about 100 to 115 1 and is usually run into pans where it is allowed to solidify. Or the melted, cacao mass is run direct from the grinding mill into agbydraulic ress, where under very heavy pressure it" oses some 60 to. 70 per cent. of the contained fat or cacao butter-.- 'The cacaoleft in the press is allowed to cool and then cruhhed,-disintegrated, and

I reduced toa fine powder, This cacao powder stillcontains a notable amount of fat and all the, other constituents of the original cacao 'rnass. II propose to. remove all ofvthe fat :andthe' alkaloids (theobromin and c'afiein) froinlthe' cacao bean, leaving all the other constituents of the-bean-in the completely fiat-tree powder, whichjconstitutes a new product of'agreeable and great nutrito be good reasons. These reasons have been 1 mainly because of difliculties in making the ertra'ction complete and because of, the persistence with which traces of the solvents ad v hered to the cacao powder left after'separa- .tion from the fat solution. v 1 I have found after long experiment with diflerent solvents under a variety of'conditions that I can effect the desired extraction of both the, fat and the alkaloids with chloroform (:a chlorinated hydrocarbon) as. the

teristic cacao served.

ducted, the pencils. will be reasonably hard into an extractor fitted over a still and prosolvent and, by reason of the method of ex tracting which I have devised, I can eficctg' I Application meantime 17,1318. s mina'zsasia the extraction with a. completeness never before attained. I am able moreover to obtain as a new and valuable product-a residual cacao-powder perfectlyfree from any trace of odor of the solvent and with the charac-.

taste and flavor fully pre-..

In carrying out my extraction and practisingrny invention I prefer to proceed as follows: The cacao beans, after cleaning, sorting and roasting, are shelled and then ground into an impalpable mass according to the general practice of the cocoa manufacturers. The resultant mass, known in the trade as liquor, is taken hot from the grinding mill and at once mixed with water (preferably hot) inthe proportion of 100 lbs. of liquor to 5.0 or '60 lbs. of water. If

the cacao po vder is to have the alkali treatinent known as ditching, a sm'all'amount of alkali may be added here in the proper-- t ions generally used for that purpose, but the alkali treatment is'not an essential part of my process and the success of my treat: merit of the cacao liquor is not dependent upon it. The hot mixture of the liquor and the water is rapidly and continuously stirred. In a short time it becomes uniformly liquid but soon, begins to set, or harden, due most probably to the swelling of the fstarchymatter in the cacao when treatedwith hot water. After the mass'has become moderately. hard but not brittle, it is made up intosmall forms such as tablets or briqucts. or molded shapes of any, convenient kind. I have found that a very suitable form is'that of long pencils or rods obtained by forcing the hardening mass through a screen with holes of about inch I d in diameter. These pencils are left in, a

warm" room provided with good ventilation,

undisturbed until most of the water has evaporated outof them, leaving from 5 to lt' per cent. only of water in the material. It the operation has been properly conwith numberless small cracks on the surface.

'In such condition I have found them to be excellently adapted for the complete extraction by the solvent.. The pencils (or dried br1quets,-1f that form he used) are now put ided witha return condenser, and the ex. ct onjwith vapor oldchloroform, is con tinned until a sample of the solvent as it.

drains from the extractor. shows complete freedom from either fat or alkaloid. Dry steam is then passed through the extractor until-all trace of the chloroform has disappeared and the contents of the ektractor are dried by warm air or bther suitable means and then emptied out; The pencils -or briquets generally hold their form throughout all this treatment but after drying they crumble on slight pressure into an impalpable powder, W ich cacao powder is now fat-free and alkaloid-free, but preserves the characteristic cacao flavor and taste and retains the nutritive value due to the carbohydrates and the proteids of the cacao-bean.

The chloroform solution is dry distilled until it reaches a temperature of 90 C. and then cooled somewhat and filtered whereby the alkaloids are separated from the melted cacao butter. The alkaloids on the filter -can be washed with a little fresh chloi'o:

form to free thernirom adhering traces of the fat and the butter is then placed in a still-and the last trace of solvent driven off 7 by free steam. The yield of cacao butter is and alkaloids, with a solvent for said fat and alkaloids until substantially all ofsaid fat; and alkaloids have'bee extraeted from said product and then driving oil the solvent ,from said fat and alkaloids.

2. The process which comprises the com bination of a cacao bean product containing fat and alkaloid, witlr'a chlorinated hydrocarbon capable of extracting said fat' and alkaloid, and driving off said chlorinated hydrocarbon from said fat and alkaloid.

3. The process which comprises the combination of a cacao bean roduct containing fat and alkaloid, with c loroform so that said 'fat and alkaloid are dissolved and drivin of? said chloroform from said fat and a1 aloid.

' 4. The fprocess which comprises the pro duction o a melted cacao mass, adding water thereto, molding and drying the product resulting from the combination of said Water with said mass, extracting fat and alka loids from said. last named product by a solvent therefor, and driving'ofi the-solvent from the fat and alkaloids.

' 5. The process which comprises the com bination with a. roasted and ground cacao mass shapes, and extracting the fat and alkaloids from said last named shapes by a'solvent.

6. Theprocess which eomprises the combination with a hot liquid cacao mass, of hot water accompanied by stirring, forming the product into suitable shapes, and extracting the cacao butterand alkaloids t-herefromiby a solvent.

7. The recess which comprises the production o a cacao wroduct containing cacao' butter and alkaloi s, treating said rodue t with a solvent (such as chloroform) f or said cacao butter and alkaloids, heating the resulting solution" so as to drive off the sub stantial art of the solvent, cooling and filtering 01? the separated alkaloids, and then drivin ofi'the last traces of the solvent.

8. T e process of obtaining thecoinbined alkaloids of the cacao bean which consists in simultaneoiisly extracting them together with the fat of the bean by means of a solvent t-herefor, then chilling the extracted alkaloids and fat until the alkaloids separate and then filtering to sephrate said alkaloids I from the fat. 9. A cacao powder containing'no fat. '10. A cacao powder containing no alkaloid.

11. A cacao powder free from fat and alkaloids. 1 j .j 12. A cacao powder free from fat and alkaloids and containing the carbohydrate and protein constituents of the cacao bean. In witness whereof I have hereuntoset my hand this twelfth day of March, 1913', 10?: in the presence of the subscribing. witnesses. I

ROBERT n. RIDDLE.

Witnesses: CHARLES H. WEISS,

' ANNA D. Game.

of hot water, molding the product into suitahle shapes for extracting, drying such 

